CN102241965B - Heat-conductive silicone grease paste and its preparation method - Google Patents

Heat-conductive silicone grease paste and its preparation method Download PDF

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CN102241965B
CN102241965B CN 201110121477 CN201110121477A CN102241965B CN 102241965 B CN102241965 B CN 102241965B CN 201110121477 CN201110121477 CN 201110121477 CN 201110121477 A CN201110121477 A CN 201110121477A CN 102241965 B CN102241965 B CN 102241965B
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heat
silicone grease
filler
preparation
paste
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CN102241965A (en
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秦如新
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Abstract

The invention discloses a heat-conductive silicone grease paste and its preparation method, and the method is characterized in that a powder filling material is mixed with aluminum nitride, zinc oxide, nanometer copper and organic silicone grease according to a certain ratio to prepare the paste. According to the invention, the nanometer level alumina coated copper powder is taken as the filling material, the prepared heat conductive silicone grease has the characteristics of no drying, no hardness and no melting under the condition of high temperature for long time, and has no flavor and no odor, no corrosion effect to metals such as iron, copper and aluminum. The invention has advantages of excellent electrical performance, insulation, moisture resistance, shock resistance, radiation resistance and aging resistance, and the heat conduction speed of the electron and electric appliance to a heat radiator can be accelerated, so that the heat radiation efficiency can be improved.

Description

A kind of heat-conducting silicone grease lotion and preparation method thereof
Technical field
The present invention relates to a kind of heat-conducting silicone grease lotion and preparation method thereof.
Background technology
Whole world illumination association is illustrated in the foreseeable future, and large-power light-emitting diodes (Powerlight-emittingdiodes) will play crucial effects in the general lighting field.Since nineteen ninety-four, great power LED obtains fast development, has replaced conventional light source at numerous areas (as street lamp, automobile tail light, LCD backlight etc.).In recent years, the development of LED technology is maked rapid progress especially, and extra large thatch (Haitz) law that is similar to Moore's Law is obeyed in the lifting of its light efficiency and the decline of device cost, and namely the LED price was reduced to originally 1/10 in per 10 years, and performance then improves 20 times.
The LED technology develops to high-power, high brightness, high-level efficiency, low-cost direction in the world.The optical characteristics of power LED and electrology characteristic depend on junction temperature strongly.Along with the increase of LED power, too high junction temperature can influence life-span and the reliability of LED, and it is increasingly serious that heat dissipation problem becomes.
The heat radiation of LED is more and more paid attention to by people now, and this is that the bad junction temperature of dispelling the heat is just high because the light decay of LED or its life-span are directly relevant with its junction temperature, and the life-span is weak point just, can prolong 2 times according to 10 ℃ of life-spans of the every reduction of A Leiniusi rule temperature.Compare with other lamp source, can produce serious heat dissipation problem, this mainly is because not by dispelling the heat.Generally speaking, the power consumption that is used for LED has 75%~85% finally to be converted to heat energy, and too much heat can reduce the light output of LED and produce colour cast, accelerates LED and wears out.If be that 25 luminous when spending are 100% with junction temperature, junction temperature rises to 60 when spending so, and its luminous quantity just has only 90%; Junction temperature is 100 just to drop to 80% when spending; 140 degree just have only 70%.As seen improve heat radiation, the control junction temperature is very important thing.The heating of LED can make that also its spectrum moves in addition; Colour temperature raises; Forward current increases (during the constant voltage power supply); Reversible circulation also increases; Variety of problems such as thermal stresses increases, thus, the heat radiation of LED is an of paramount importance problem in the design of LED light fixture.The characteristics of led chip are at the high heat of minimum volume generation.And the thermal capacity of LED itself is very little, thus must conduct these heats with the fastest speed, otherwise will produce very high junction temperature.After the led chip encapsulation, the thermal resistance from the chip to the pin is exactly a most important thermal resistance when using, and in general, the size of the face that the connects area of chip is the key of heat radiation, for different rated output, requires to have the face that the connects area of corresponding size.
Use the better heat abstractor of thermal conductivity, be decreased to the thermal resistance of environment, control LED internal temperature is unlikely high more too many than envrionment temperature, but this needs higher cost.In addition, the problem that is difficult to avoid is, radiator element at the lamp body shell after heat abstractor uses for some time deposits dust, and aging the coming unstuck of medium layer that connects copper layer and aluminium base on the Al-alloy based copper clad plate all will cause thermal resistance to rise greatly, causes the integral heat sink degradation.
Summary of the invention
In order to reach less thermal resistance, improve the purpose of thermal conductivity, the invention provides a kind of heat-conducting silicone grease lotion and preparation method thereof.
The present invention adopts following technical scheme to achieve these goals:
The heat-conducting silicone grease lotion is characterized in that the weight ratio of its constitutive material is: powder filler 10-75%, aluminium nitride 5-45%, zinc oxide 0-10%, organic silicone grease 15-30%, nanometer copper 1-20%.
Described heat-conducting silicone grease lotion is characterized in that described powder filler is the alumina powder jointed filler of cupric 20%.
The preparation method of described heat-conducting silicone grease lotion is characterized in that may further comprise the steps:
(1) preparation powder filler: with AI (NO 3) 3.9HO with citric acid in molar ratio 1: the 1.2-1.5 proportioning is soluble in water, uses dense HNO 3Or dense NH 3H 2The O regulator solution is 3-4 to PH, gets colourless transparent solution, adds nanometer copper by the weight ratio of raw material then and is uniformly dispersed, and after filtration, evaporation, vacuum-drying, at 550-580 ℃ of roasting 10h, gets the alumina powder jointed filler of cupric 20%;
(2) will make powder filler, aluminium nitride, zinc oxide, organic silicone grease, nanometer copper by oneself by the weight ratio of raw material and add kneader and under the kneading state, mix, make the paste heat-conducting cream.
Beneficial effect of the present invention:
It is filler that the present invention adopts alumina in Nano level to coat copper powder, and the heat-conducting silicone grease of preparation has at long-time 280 ℃, in addition the high temperature more than 280 ℃ reveal put also do not do, not hard, insoluble, and tasteless, odorless does not all have corrosive nature to metals such as iron, copper, aluminium; Have excellent electric property, insulation, moistureproof, shockproof, radiation hardness is aging etc., and can accelerate electronics, electrical equipment to the heat conduction velocity of heat abstractor, thereby the characteristics of raising radiating efficiency.
Embodiment
Preparation powder filler: with AI (NO 3) 3.9HO with citric acid in molar ratio 1: the 1.2-1.5 proportioning is soluble in water, uses dense HNO 3Or dense NH 3H 2The O regulator solution is 3-4 to PH, gets colourless transparent solution, adds nanometer copper by the weight ratio of raw material then and is uniformly dispersed, and after filtration, evaporation, vacuum-drying, at 550-580 ℃ of roasting 10h, gets the alumina powder jointed filler of cupric 20%, and is stand-by;
Embodiment 1
Earlier each component is mediated in kneader by following prescription (mass parts), disperse at three-roll grinder then, mix and make the paste heat-conducting cream.
Powder filler 75%
Organic silicone grease 25%
Embodiment 2
Earlier each component is mediated in kneader by following prescription (mass parts), disperse at three-roll grinder then, mix and make the paste heat-conducting cream.
Powder filler 52%
Aluminium nitride 25%
Organic silicone grease 23%
Embodiment 3
Earlier each component is mediated in kneader by following prescription (mass parts), disperse at three-roll grinder then, mix and make the paste heat-conducting cream.
Figure BDA0000060606210000031
Embodiment 4
Earlier each component is mediated in kneader by following prescription (mass parts), disperse at three-roll grinder then, mix and make the paste heat-conducting cream.
Figure BDA0000060606210000032
Embodiment 5
Earlier each component is mediated in kneader by following prescription (mass parts), disperse at three-roll grinder then, mix and make the paste heat-conducting cream.
Embodiment 6
Earlier each component is mediated in kneader by following mass parts, disperse at three-roll grinder then, mix and make the paste heat-conducting cream: powder filler 45%, aluminium nitride 25%, zinc oxide 5%, organic silicone grease 15%, nanometer copper 10%.
More than the prepared heat-conducting cream of each embodiment be the thermal conduction chemicals, can maximize the thermal conduction between semiconductor piece and the scatterer; Be exposed to for a long time under the hot environment and also can not harden; Environment-protecting asepsis; Have remarkable electrical insulation capability, but automated operation and silk screen printing.All can reach heat-conduction coefficient ThermalConductivity>4.5W/M.K thermal impedance Thermal Impedance<0.067 ℃-in2/W.

Claims (2)

1. a heat-conducting silicone grease lotion is characterized in that the weight ratio of its constitutive material is: powder filler 10-75%, aluminium nitride 5-45%, zinc oxide 0-10%, organic silicone grease 15-30%, nanometer copper 1-20%; Described powder filler is the alumina powder jointed filler of cupric 20%.
2. the preparation method of heat-conducting silicone grease lotion according to claim 1 is characterized in that may further comprise the steps:
(1) preparation powder filler: with Al (NO 3) 3`9H 2The 1:1.2-1.5 proportioning is soluble in water in molar ratio for O and citric acid, uses dense HNO 3Or dense NH 3H 2The O regulator solution is 3-4 to pH, gets colourless transparent solution, adds nanometer copper by the weight ratio of raw material then and is uniformly dispersed, and after filtration, evaporation, vacuum-drying, at 550-580 ℃ of roasting 10h, gets the alumina powder jointed filler of cupric 20%;
(2) will make powder filler, aluminium nitride, zinc oxide, organic silicone grease, nanometer copper by oneself by the weight ratio of raw material and add kneader and under the kneading state, mix, make the paste heat-conducting cream.
CN 201110121477 2011-05-12 2011-05-12 Heat-conductive silicone grease paste and its preparation method Expired - Fee Related CN102241965B (en)

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CN102241965B true CN102241965B (en) 2013-08-07

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Publication number Priority date Publication date Assignee Title
CN103772993A (en) * 2014-01-26 2014-05-07 一远电子科技有限公司 High thermal conductivity nano-copper heat conducting silicon grease and preparation method thereof
CN104974555A (en) * 2015-06-27 2015-10-14 铜陵铜基粉体科技有限公司 Spherical copper powder with corrosion resistance and excellent thermal stability, and preparation method thereof
CN105524550A (en) * 2016-01-22 2016-04-27 何挺 Heat-conducting silicone grease and manufacturing method thereof
CN110358146A (en) * 2018-04-10 2019-10-22 博世汽车部件(苏州)有限公司 The copper nano-wire of alumina-coated, heat conductive silica gel and preparation method thereof
CN109659281B (en) * 2019-01-29 2020-05-01 中南大学 High-thermal-conductivity electronic packaging composite material and preparation method thereof

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JP5372388B2 (en) * 2008-01-30 2013-12-18 東レ・ダウコーニング株式会社 Thermally conductive silicone grease composition

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